CN108663387B - Method for preparing nano-particle TEM sample by wet etching - Google Patents
Method for preparing nano-particle TEM sample by wet etching Download PDFInfo
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Abstract
The invention provides a method for preparing a nano-particle TEM sample by wet etching. The method for preparing the nano-particle TEM sample by wet etching comprises the following steps: 1) horizontally placing a TEM supporting film, and dripping an etching agent on the TEM supporting film; 2) inverting the substrate adhered with the nanoparticles to ensure that one surface of the substrate with the nanoparticles to be transferred faces downwards and gradually contacts with an etchant, and separating the etched nanoparticles to be transferred from the substrate and transferring the etched nanoparticles to a TEM support film; 3) and standing the TEM support film until the etching agent is volatilized, and finishing the sample preparation of the nano-particle TEM sample. The method for preparing the nano-particle TEM sample by wet etching has low cost and high efficiency, can completely transfer the nano-particles adhered to the substrate onto the TEM supporting film, has no agglomeration and no damage of the transferred nano-particles, and is convenient for the performance characterization of high-resolution lattices and the like of the nano-particle TEM sample.
Description
Technical Field
The invention belongs to the technical field of microscopic detection of a transmission electron microscope, and relates to a method for preparing a nano-particle TEM sample by wet etching.
Background
With the development of nano science and technology, nanowires, quantum dots, nano films and the like are widely applied in the fields of micro-nano electronics, nano optics, reaction catalysis and the like. The material characteristic analysis of the nano-structure with the dimension of 0.1-100 nm is the premise of various applications. Among them, Transmission Electron Microscopy (TEM) plays an irreplaceable role in the characterization of lattice structure, elemental composition, electron distribution, etc., with high resolution on the order of sub-angstroms.
The method uses high-energy beam and plasma from top to bottom, can directly prepare large-area nano particles with the size less than 50nm or other fine nano structures on a nano film supported by a substrate, and is widely and importantly applied in the fields of biological detection, imaging, sensing and the like. Unlike self-assembled structures, the nanostructures on these films adhere strongly to the substrate, which brings about a challenge to TEM sampling and characterization of the nanostructures while bringing extremely high device stability.
In practice, for the nanoparticle sample less than 50nm that is tightly adhered to the substrate, the conventional sampling methods include ion thinning, FIB (focused ion beam) sampling, mechanical (knife) transfer, and the like. However, these conventional sample preparation methods have many disadvantages, for example, ion thinning may damage the nanoparticles; FIB (focused ion beam) sample preparation has the defects of sample pollution, difficulty in obtaining complete nano particles and the like; the mechanical (knife) transfer method can cause severe agglomeration of particles, etc.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing a nano-particle TEM sample by wet etching, which has low cost and high efficiency, can completely transfer nano-particles adhered to a substrate onto a TEM supporting film, has no agglomeration and no damage of the transferred nano-particles, and is convenient for performance characterization of high-resolution lattices and the like of the nano-particle TEM sample.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a nano-particle TEM sample by wet etching comprises the following steps:
1) horizontally placing a TEM supporting film, and dripping an etching agent on the TEM supporting film;
2) inverting the substrate adhered with the nanoparticles to ensure that one surface of the substrate with the nanoparticles to be transferred faces downwards and gradually contacts the etchant in the step 1), and separating the etched nanoparticles to be transferred from the substrate and transferring the nanoparticles to a TEM support film;
3) and (3) standing the TEM support film in the step 2) until the etching agent is volatilized, and finishing the sample preparation of the nano-particle TEM sample.
Preferably, the following steps are further included between step 1) and step 2): and covering and shielding the area except the nano particles to be transferred on the substrate.
Preferably, the tape is used to cover and shield the substrate except the region to be transferred with the nanoparticles. And selecting a target area to be transferred, and covering and shielding the part outside the target area by using a clean adhesive tape which does not react with the etching agent so as to realize accurate area selection sample transfer. This step can be omitted if selective sample transfer is not required.
The etchant should satisfy the following conditions: the etchant does not react with the nanoparticles and the TEM support film but can react with the substrate to etch and avoid introducing impurities as much as possible during the reaction. For example, the substrate is silicon dioxide, the TEM support film is a carbon film, the nanoparticle sample is silver nanoparticles, and hydrofluoric acid is selected as the etchant.
The etchant is one of hydrofluoric acid, nitric acid, sulfuric acid and acetone, but is not limited to the etchant, and can also be commonly used etchant such as other acids. The amount of etchant used depends on the region of the nanoparticle to be transferred, and the choice of etchant also depends on the substrate material and the type of nanoparticle to be transferred.
Preferably, the mass concentration of the etchant is 1-30%, for example, the mass concentration of the etchant is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%. The mass concentration of the etching agent influences the sample preparation efficiency and the sample preparation effect, and if the mass concentration of the etching agent is lower than 1%, the etching time is too long, and the stripping of an etching area is incomplete; if the mass concentration of the etchant is higher than 30%, the etching rate is too fast, and it is difficult to control the experimental time.
The nanoparticles have a particle size of 50nm or less, for example, 1nm, 5nm, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, or 50 nm.
The nanoparticles are metal nanoparticles; preferably, the metal nanoparticles are noble metal nanoparticles.
The substrate is a silicon wafer, a glass sheet or a plastic sheet.
The TEM support film is a support film commonly used for transmission electron microscopy, such as a copper mesh support film, a carbon support film, a silicon nitride support film, a silicon oxide support film and the like.
As a preferable scheme, the method for preparing the nano-particle TEM sample by wet etching comprises the following steps:
1) horizontally placing a TEM support film, and dripping an etchant with the mass concentration of 1-30% on the TEM support film;
2) inverting the substrate adhered with the nanoparticles with the particle size of below 50nm to enable one surface of the substrate with the nanoparticles to be transferred to face downwards and gradually contact the etching agent in the step 1), and enabling the etched nanoparticles to be transferred to be separated from the substrate and transferred to a TEM support film;
3) and (3) standing the TEM support film in the step 2) until the etching agent is volatilized, and finishing the sample preparation of the nano-particle TEM sample.
As a further preferred scheme, the method for preparing the nano-particle TEM sample by wet etching of the invention comprises the following steps:
1) horizontally placing a TEM support film, and dripping hydrofluoric acid on the TEM support film;
2) inverting the glass substrate adhered with the silver nanoparticles with the particle size of below 50nm to enable one surface of the substrate, which is provided with the target area to be transferred, of the nanoparticles to be transferred to face downwards and gradually contact the hydrofluoric acid in the step 1), and enabling the etched nanoparticles to be transferred to be separated from the substrate and transferred to a TEM support film;
3) standing the TEM support film obtained in the step 2) until hydrofluoric acid is volatilized, and finishing sample preparation of the silver nanoparticle TEM sample.
As a further preferable scheme, the method for preparing the nano-particle TEM sample by wet etching comprises the following steps:
1) horizontally placing a TEM support film, and dripping hydrofluoric acid on the TEM support film;
2) covering and shielding the area outside the nano particles to be transferred on the glass substrate by using an adhesive tape;
3) inverting the glass substrate adhered with the silver nanoparticles with the particle size of below 50nm to enable one surface of the substrate, which is provided with the target area to be transferred, of the nanoparticles to be transferred to face downwards and gradually contact the hydrofluoric acid in the step 1), and enabling the etched nanoparticles to be transferred to be separated from the substrate and transferred to a TEM support film;
4) standing the TEM support film obtained in the step 3) until the hydrofluoric acid is volatilized, and finishing the sample preparation of the silver nanoparticle TEM sample.
Compared with the prior art, the invention has the beneficial effects that:
the method for preparing the nano-particle TEM sample by wet etching has low cost and high efficiency, can completely transfer the nano-particles adhered to the substrate onto the TEM supporting film, has no agglomeration phenomenon of the transferred nano-particles, has no damage to the transferred nano-particles, maintains the original appearance of the nano-particles, and is convenient for performance characterization such as high-resolution crystal lattices of the nano-particle TEM sample.
Drawings
FIG. 1 is a process flow diagram of a method of wet etching a TEM sample of nanoparticles according to the invention;
FIG. 2 is a schematic diagram of a method of wet etching a TEM sample of nanoparticles according to the invention; the method comprises the following steps of A-a sample substrate, B-a target sample to be transferred and characterized on the sample substrate, C-an etchant droplet, D-a TEM support film, the state of an E-sample when contacting with an etchant, the sample substrate after F-transfer is finished, and G-a prepared TEM sample;
FIG. 3 is a schematic diagram of a sample after being subjected to a precise region selection treatment in the preparation method of the present invention; wherein, A ' -an adhesive tape for shielding a non-target area, B ' -a target sample area to be transferred and C ' -a glass slide;
FIG. 4 is an SEM topography characterization image of a sample prepared by the preparation method of example 1 of the present invention; wherein, A-the silver particle sample after transfer, B-TEM support film;
FIG. 5 is a TEM image of individual silver nanoparticles of 13nm in size for the sample of FIG. 4; wherein, A-the transferred silver particles, B-TEM support film;
FIG. 6 is a TEM image of a single silver nanoparticle having a particle size of 25nm of a sample prepared by the preparation method of example 2 of the present invention; wherein, A-the transferred silver particles, B-TEM support film;
FIG. 7 is an SEM topography characterization image of a sample prepared by the knife scraping method of a comparative example of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached figures 1-7.
The process flow diagram of the method for preparing the nano-particle TEM sample by wet etching is shown in FIG. 1, the method for preparing the TEM sample by micro wet etching is particularly suitable for the nano-particle sample adhered on a substrate, and comprises the following steps:
firstly, selecting an etching agent according to the material properties of a nanoparticle sample, an attached substrate and a TEM support film;
secondly, covering and shielding the area outside the target transfer area of the sample by using a clean adhesive tape as required;
thirdly, horizontally placing the TEM supporting film, and dripping a proper amount of etchant on the TEM supporting film;
fourthly, the sample surface is completely contacted with the etching agent, and the nano particles fall off to the TEM supporting film to finish the transfer;
and fifthly, obtaining a needed TEM detection sample after the etching agent is completely volatilized.
FIG. 2 is a schematic representation of a sample preparation method of the present invention. Wherein, A is a substrate of a sample, B is a target sample to be transferred and characterized on the sample substrate, C is a selected etchant droplet, D is a TEM support film, E is a state when the sample is in contact with the etchant, F is the sample substrate after the transfer is finished, and G is a TEM sample which is successfully prepared.
FIG. 3 is a schematic diagram of a sample after being subjected to a precise region selection treatment in the preparation method of the present invention; wherein, A ' -an adhesive tape for shielding a non-target area, B ' -a target sample area to be transferred and C ' -a glass slide; if only the sample of the target area needs to be transferred, rather than the whole sample, the adhesive tape can be used to cover and shield the area outside the nanoparticles to be transferred on the silica substrate, so as to accurately determine the sample to be transferred in the selected area.
Example 1
The invention takes silver nano particles with the particle size of 13nm adhered on a silicon dioxide substrate as an example, the sample preparation is carried out according to the specific steps in the invention, the TEM supporting film is a carbon film, and the etchant selects a hydrofluoric acid solution with the concentration of 5%.
FIG. 4 is an SEM topography representation image of a sample prepared by the preparation method of this example; wherein A is the silver particle sample after transfer, and B is a TEM support film. As can be seen from fig. 4, the silver nanoparticle sample was completely transferred to the TEM support film, and the silver nanoparticles did not aggregate.
FIG. 5 is a TEM image of individual silver nanoparticles of the sample of FIG. 4; wherein A is the transferred silver particles and B is a TEM support film. As can be seen from the high resolution lattice characterization of fig. 5, the method of the present invention can effectively transfer nanoparticles without damage to the nanoparticles, and maintains the original morphology of the silver nanoparticles.
Example 2
Taking a single silver nanoparticle with the particle size of 25nm adhered on a silicon dioxide substrate as an example, the sample preparation is carried out according to the specific steps in the invention, the TEM supporting film is a carbon film, and the etchant is a hydrofluoric acid solution with the concentration of 5%.
Fig. 6 is a TEM image of a single silver nanoparticle having a particle size of 25nm after being transferred according to the above-described method, and it can be seen from fig. 6 that a sample of a single silver nanoparticle having a particle size of 25nm is completely transferred onto a TEM supporting film and the aggregation of the silver nanoparticles does not occur.
Example 3
The invention takes gold nanoparticles with the particle size of 13nm adhered on a silicon dioxide substrate as an example, the sample preparation is carried out according to the specific steps in the invention, the TEM supporting film is a copper net supporting film, and hydrofluoric acid solution with the concentration of 1% is selected as an etching agent.
The SEM morphology characterization of the sample prepared by the preparation method of this example shows that the gold nanoparticle sample is completely transferred to the TEM support film and that no agglomeration of the gold nanoparticles occurs.
Example 4
The invention takes silver nano-particles with the particle size of 45nm adhered on a plastic sheet substrate as an example, the sample preparation is carried out according to the specific steps in the invention, the TEM supporting film is a silicon nitride supporting film, and the etchant selects a sulfuric acid solution with the concentration of 25%.
The SEM morphology characterization of the sample prepared by the preparation method of this example shows that the silver nanoparticle sample is completely transferred to the TEM support film and that the silver nanoparticles do not agglomerate.
Example 5
The invention takes silver nano particles with the particle size of 20nm adhered on a silicon chip substrate as an example, the sample preparation is carried out according to the specific steps in the invention, the TEM supporting film is a silicon oxide supporting film, and the etching agent selects acetone solution with the concentration of 30 percent.
The SEM morphology characterization of the sample prepared by the preparation method of this example shows that the silver nanoparticle sample is completely transferred to the TEM support film and that the silver nanoparticles do not agglomerate.
Comparative example
For the nanoparticle sample attached to the substrate, knife scraping is another common method for TEM sampling, but this method is not suitable for high surface energy nanoparticles with a particle size below 50nm attached to the substrate, because of severe agglomeration.
Fig. 7 is Ag nanoparticles transferred to a TEM carbon support film using the knife-scraping method, and it can be seen from fig. 7 that severe agglomeration of the samples made using the knife-scraping method resulted in failure to characterize individual Ag nanoparticles.
The above examples are only intended to illustrate the detailed process of the present invention, and the present invention is not limited to the above detailed process, i.e., it is not intended that the present invention necessarily depends on the above detailed process for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (7)
1. A method for preparing a nano-particle TEM sample by wet etching is characterized by comprising the following steps:
1) horizontally placing a TEM supporting film, and dripping an etching agent on the TEM supporting film;
2) inverting the substrate adhered with the nanoparticles, so that one surface of the substrate with the nanoparticles to be transferred faces downwards and gradually contacts with the etchant in the step 1), separating the etched nanoparticles to be transferred from the substrate and transferring the etched nanoparticles to a TEM support film, wherein the etchant is an etchant which does not react with the nanoparticles and the TEM support film and is etched in a reaction manner with the substrate, the etchant is one of hydrofluoric acid, nitric acid and sulfuric acid, the mass concentration of the etchant is 1-30%, the nanoparticles are metal nanoparticles, and the particle size of the nanoparticles is less than 50 nm; the substrate is a silicon wafer, a glass sheet or a plastic sheet;
3) and (3) standing the TEM support film in the step 2) until the etching agent is volatilized, and finishing the sample preparation of the nano-particle TEM sample.
2. The method according to claim 1, characterized by further comprising the following steps between the step 1) and the step 2): and covering and shielding the area except the nano particles to be transferred on the substrate.
3. The method of claim 2, wherein the tape is used to cover areas of the substrate other than the nanoparticles to be transferred.
4. The method of claim 1, wherein the nanoparticles are noble metal nanoparticles.
5. The method of claim 1, wherein the TEM support film is a copper mesh support film, a carbon support film, a silicon nitride support film, or a silicon oxide support film.
6. Method according to claim 1, characterized in that it comprises the following steps:
1) horizontally placing a TEM support film, and dripping hydrofluoric acid on the TEM support film;
2) inverting the glass substrate adhered with the silver nanoparticles with the particle size of below 50nm to enable one surface of the substrate, which is provided with the target area to be transferred, of the nanoparticles to be transferred to face downwards and gradually contact the hydrofluoric acid in the step 1), and enabling the etched nanoparticles to be transferred to be separated from the substrate and transferred to a TEM support film;
3) standing the TEM support film obtained in the step 2) until hydrofluoric acid is volatilized, and finishing sample preparation of the silver nanoparticle TEM sample.
7. Method according to claim 1, characterized in that it comprises the following steps:
1) horizontally placing a TEM support film, and dripping hydrofluoric acid on the TEM support film;
2) covering and shielding the area outside the nano particles to be transferred on the glass substrate by using an adhesive tape;
3) inverting the glass substrate adhered with the silver nanoparticles with the particle size of below 50nm to enable one surface of the substrate, which is provided with the target area to be transferred, of the nanoparticles to be transferred to face downwards and gradually contact the hydrofluoric acid in the step 1), and enabling the etched nanoparticles to be transferred to be separated from the substrate and transferred to a TEM support film;
4) standing the TEM support film obtained in the step 3) until the hydrofluoric acid is volatilized, and finishing the sample preparation of the silver nanoparticle TEM sample.
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